Method for preparing magnesium hydroxide flame retardant by microchannel precipitation-hydrothermal process

A technology of magnesium hydroxide and flame retardant, applied in the direction of magnesium hydroxide, etc., to achieve the effects of controllable particle size, reduction of system energy consumption and complexity, and continuous reaction process

Active Publication Date: 2015-03-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the above public information, magnesium hydroxide with two extreme particle sizes greater than 1 μm and less than 0.1 μm was prepared by using a microchannel reactor, and the controllable preparation of submicron hexagonal flake-shaped magnesium hydroxide particles is a difficult point in research. From According to literature search, the microchannel synthesis technology of submicron hexagonal flake magnesium hydroxide flame retardant is still in the blank

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  • Method for preparing magnesium hydroxide flame retardant by microchannel precipitation-hydrothermal process
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  • Method for preparing magnesium hydroxide flame retardant by microchannel precipitation-hydrothermal process

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Embodiment 1

[0033] A 1.0 mol / L magnesium chloride solution and a 1.0 mol / L sodium hydroxide solution were prepared, and the two raw material solutions were respectively pumped to the microchannel reactor at room temperature. Wherein the pump speed of magnesium chloride solution is controlled at 50ml / min, and the pump speed of sodium hydroxide solution is controlled at 110ml / min, and the precipitation reaction mol ratio n (Mg 2+ ) / n(OH - ) is 1:2.2. The slurry at the outlet of the microchannel reactor directly enters the hydrothermal synthesis kettle, the hydrothermal reaction temperature is 150° C., and the hydrothermal time is 2 hours. The product after hydroheating is cooled, filtered, washed (detected by silver nitrate until no chloride ion is detected), dried at 110°C for 10 hours, and crushed to obtain a particle size of 100-200nm, a purity of 99.1%, and a specific surface area of ​​17.6m 2 / g of hexagonal flake magnesium hydroxide. The SEM picture of the product is attached fig...

Embodiment 2

[0035]A 2.0 mol / L magnesium chloride solution and a 2.0 mol / L sodium hydroxide solution were prepared, and the two raw material solutions were respectively pumped to the microchannel reactor at room temperature through advection pumping. Wherein the pump speed of magnesium chloride solution is controlled at 20ml / min, and the pump speed of sodium hydroxide solution is controlled at 50ml / min, and the precipitation reaction mol ratio n (Mg 2+ ) / n(OH - ) is 1:2.5. The slurry at the outlet of the microchannel reactor directly enters the hydrothermal synthesis kettle, the hydrothermal reaction temperature is 160° C., and the hydrothermal time is 4 hours. The product after hydroheating is cooled, filtered, washed (detected by silver nitrate until no chloride ion is detected), dried at 110°C for 10 hours, and crushed to obtain a particle size of 200-300nm, a purity of 98.6%, and a specific surface area of ​​13.2m 2 / g of hexagonal flake magnesium hydroxide. The SEM picture of the p...

Embodiment 3

[0037] A 3.0 mol / L magnesium chloride solution and a 6.0 mol / L sodium hydroxide solution were prepared, and the two raw material solutions were respectively pumped to the microchannel reactor at room temperature. Wherein the pump speed of magnesium chloride solution is controlled at 160ml / min, and the pump speed of sodium hydroxide solution is controlled at 120ml / min, and the precipitation reaction mol ratio n (Mg 2+ ) / n(OH - ) is 1:1.5. The slurry at the outlet of the microchannel reactor directly enters the hydrothermal synthesis kettle, the hydrothermal reaction temperature is 180° C., and the hydrothermal time is 4 hours. The product after hydroheating is cooled, filtered, washed (detected by silver nitrate until no chloride ion is detected), dried at 110°C for 10 hours, and crushed to obtain a particle size of 400-600nm, a purity of 99.0%, and a specific surface area of ​​11.8m 2 / g of hexagonal flake magnesium hydroxide. The SEM picture of the product is attached Fi...

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Abstract

The invention provides a method for preparing a magnesium hydroxide flame retardant by a microchannel precipitation-hydrothermal process, which comprises the following steps: + continuously mixing a magnesium chloride solution and a sodium hydroxide solution in a microchannel reactor, and carrying out precipitation reaction in the microchannel reactor at room temperature; after the reaction slurry continuously flows out of the microchannel reactor, carrying out hydrothermal reaction at 150-200 DEG C for 2-6 hours, filtering, washing and drying to obtain the high-purity hexagonal flaky magnesium hydroxide flame retardant. The method has the advantages of continuous reaction process, simple technical process, no scale-up effect and the like; and the obtained product has the advantages of controllable particle size, narrow particle size distribution, regular shape and high purity.

Description

technical field [0001] The invention belongs to the technical fields of material chemistry and inorganic chemical industry, and relates to a preparation method of a magnesium hydroxide flame retardant, in particular to a method for preparing inorganic submicron magnesium hydroxide by utilizing liquid-liquid direct precipitation reaction in a microchannel reactor flame retardant method. Background technique [0002] As an important inorganic chemical product, magnesium hydroxide has a wide range of uses in the fields of materials, chemicals, and environmental protection. As an inorganic flame retardant, it has high decomposition temperature, good smoke suppression effect, no toxic gas, and no corrosion itself. Etc. Magnesium hydroxide used as a flame retardant requires small particle size, narrow particle size distribution, flake or needle shape, high purity, and good crystallinity, among which particle size and particle size distribution are key indicators. The smaller the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F5/22
Inventor 陈光文任明月李淑莲赵玉潮杨梅
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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